반응 #72718

ord-35b8cd1e5e834e47815816d05cce98c3

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction mixture was quenched by addition of 1 M HCl (50 ml)
  2. 2
    workup.ADDITIONThen, the mixture was basified by addition of NaOH (1M aqueous solution)
  3. 3
    기타the resulted layers were separated
  4. 4
    추출This aqueous phase was extracted with CH2Cl2
  5. 5
    건조dried over MgSO4
  6. 6
    기타finally the solvents were removed under reduced pressure

실험 절차

A solution of 22 (12 mmol) in tetrachloroethane was added to the suspension of AlCl3 (36 mmol) in tetrachloroethane (50 ml). The resulting mixture was heated to 60° C. for 1.5 hrs. The reaction mixture was quenched by addition of 1 M HCl (50 ml). Then, the mixture was basified by addition of NaOH (1M aqueous solution), the resulted layers were separated, and the aqueous layer was acidified by HCl (aqueous solution). This aqueous phase was extracted with CH2Cl2, dried over MgSO4 and finally the solvents were removed under reduced pressure, to give 35% yield of the desired product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541428B2uspto-grants-2013_09